摘要
建立了加速溶剂萃取／高效液相色谱-质谱法（ASE／HPLC—MS）测定毛冬青药材中活性成分ilexgenin A和ilexsaponin A1含量的方法。采用ASE萃取毛冬青药材中的活性成分ilexgenin A和ilexsaponin A1，萃取溶剂为甲醇，萃取温度100℃，压力1．0×10^7 Pa，静态萃取模式，循环3次，每次萃取10min。采用HPLC—MS对萃取液中ilexgenin A和ilexsaponin A1进行定量分析，色谱柱选用Dikma Diamonsil C18（4．6mm×250mm，5μm），以水和乙腈为流动相进行梯度洗脱，大气压化学电离源（APCI），定量离子m／z485。ilexgenin A和ilexsaponin A1的线性范围为1．0～200．0mg／L，对毛冬青试样的定量下限分别为19．5和35．0μg/g，RSD分别为6．7％和7．8％，回收率分别为87％～96％和93％-102％。将建立的方法用于分析11个不同产地的毛冬青药材，ilexgenin A含量为0．42～6．3mg／g，ilexsaponin A1含量为0．80～8．9mg／g。
A method for determination of ilexgenin A and ilexsaponin A1 in Radix Ilicis Pubescentis by accelerated solvent extraction（ASE） followed with high performance liquid chromatography-mass spectrometry（HPLC- MS） was developed. The samples were extracted by ASE for 10 min × 3 at temperature of 100 ℃ and pressure of 1.0 × 107 Pa, with methanol as extraction solvent. The extract were separated on a Dikma Diamonsil C18 column（4. 6 mm ℃250 mm, 5 μm） with water-acetonitrile as mobile phase and detected by APCI - MS using m/z 485 as quantitative ion. The linearity ranges were both from 1.0 to 200.0 mg/L. The quantitation limits were 19.5 μg/g for ilexgenin A and 35.0 μg/g for ilexsaponin A1, with RSD of 6.7% for ilexgenin A and 7.8% for ilexsaponin A1. The recoveries ranged from 87% to 96% for ilexgenin A and from 93% to 102% for ilexsaponin A1. The method was applied to the determination of 11 Radix Ilicis Pubescentis from different producing areas, the concentrations ranged from 0. 42 to 6.3 mg/g for ilexgenin A and from 0. 80 to 8. 9 mg/g for ilexsaponin A1, respectively. The method is simple, fast, efficient and meet the requirements of the quality control of Radix Ilicis Pubescentis herbs.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第8期966-969,共4页
Journal of Instrumental Analysis
基金
广东省科技计划资助项目(2007B031407006)
广州市科技计划资助项目(2008Z1-E341)
